Determination of oxygen content in ultrafine copper powder by electron probe microanalysis
LIU Ying1, ZHANG Xungao1,2*
1. Centre for Analysis and Measurement,Wuhan University, Wuhan 430072, China; 2. Centre for Analysis and Measurement,Tarim University, Alaer 843300, China
Abstract：The degree of oxidation of ultrafine copper powder decides the performance and application of products. Rapid and accurate determination of O content in ultrafine copper powder has important practical significance. In experiments, the sample was prepared by pressed powder pellet method using self-made aluminum mold. The powder of CuO, Cu2O and Cu with particle size less than 10 μm was selected to represent ultrafine copper powder with high, medium, and low content of O, respectively. The content of O in ultrafine copper powder was quantitatively analyzed by electron probe microanalysis (EPMA) . The linear range of beam for quantitative analysis of O and Cu was investigated when the acceleration voltage was 15 kV. The effect of analytical line of Cu, beam current, and beam spot size on the quantitative analysis of O was discussed. The results showed that Cu Kα line had better quantitative effect than Lα line. The optimal linear range of beam current and beam spot size were 5-100 nA and 50 μm, respectively. Under the optimal measuring conditions, the relative standard deviations (RSD, n=9) of measurement results of high, medium, and low content of O in copper powder were all not more than 3.0%. The limit of detection of O was 0.042%. The relative error of O in standard sample of Cu2O was -4.11%. Compared to the measurement results of hydrogen loss method, the relative error of O in CuO and Cu powder samples was -5.95% and -7.04%, respectively.
[1] 牛雨萌,赖奕坚,赵斌元,等. 微纳米铜粉的制备工艺与应用特性[J].功能材料,2018,49(5):05041-05048. NIU Yumeng,LAI Yijian,ZHAO Binyuan,et al.Preparation and characterization of copper powder particles[J].Functional Materials,2018,49(5):05041-05048. [2] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 5158.3—2011 金属粉末 还原法测定氧含量 第3部分:可被氢还原的氧[S].北京:中国标准出版社,2011. [3] 何英.提高脉冲库仑法钽丝中氧检测精度的研究[J].稀有金属与硬质合金,2009,37(4):41-43. HE Ying.Improvement in the oxygen measurement precision by pulsed coulometry from tantalum wires [J].Rare Metals and Cemented Carbides,2009,37(4):41-43. [4] 侯桂臣,张琳,李一懿,等. “直投法”应用于金属粉末样品中氧氮氢分析[J].冶金分析,2019,39(6):7-13. HOU Guichen,ZHANG Lin,LI Yiyi,et al.Application of “direct-dropping” for analysis of oxygen,nitrogen and hydrogen in metal powder sample [J].Metallurgical Analysis,2019,39(6):7-13. [5] 王学华,杨植岗,王蓬,等.惰气熔融-红外吸收法测定硅钙合金中氧[J].冶金分析,2017,37(4):53-56. WANG Xuehua,YANG Zhigang,WANG Peng,et al.Determination of oxygen in silicon-calcium alloy by inert gas fusion infrared absorption method[J].Metallurgical Analysis,2017,37(4):53-56. [6] 张迪,陈意,毛骞,等.电子探针分析技术进展及面临的挑战[J].岩石学报,2019,35(1):261-274. ZHANG Di,CHEN Yi,MAO Qian,et al.Progress and challenge of electron probe microanalysis technique[J].Acta Petrologica Sinica,2019,35(1):261-274. [7] 杨琴,杨勇,宋俊磊.电子探针定量分析测定FeO和Fe2O3含量常用方法的评定[J].岩矿测试,2007,26(3):213-218. YANG Qin,YANG Yong,SONG Junlei.Evaluation of the methods for quantitative determination of FeO and Fe2O3 by electron probe microanalysis[J].Rock and Mineral Analysis,2007,26(3):213-218. [8] 张文兰,车旭东,王汝成,等.超轻元素铍的电子探针定量分析最佳条件探索:以绿柱石为例[J].科学通报,2020,65(28-29):3205-3216. ZHANG Wenlan,CHE Xudong,WANG Rucheng,et al.Optimum conditions for quantitative analysis of beryllium by electron probe microanalysis:A case study of beryl[J].Chinese Science Bulletin,2020,65(28-29):3205-3216. [9] Jonnard P,Brisset F,Robaut F,et al.Inter-laboratory comparison of a WDS-EDS quantitative X-ray microanalysis of a metallic glass[J].X-Ray Spectrometry,2015,44(1):24-29. [10] 刘英,张勋高.能谱定量分析不确定的评估[J].分析仪器,2021(1):23-32. LIU Ying,ZHANG Xungao.Uncertainty evaluation for quantitative analysis by energy dispersive spectroscopy[J].Analytical Instrumentation,2021(1):23-32. [11] 谢忠信,赵宗铃,张玉斌,等. X射线光谱分析[M].北京:科学出版社,1982:171. [12] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 17359—2012 微束分析 能谱法定量分析[S].北京:中国标准出版社,2012. [13] 周剑雄,毛水和.电子探针分析[M].北京:地质出版社,1988:162.
